CN112021318A - Annular pesticide slow-release agent and preparation method and application thereof - Google Patents

Annular pesticide slow-release agent and preparation method and application thereof Download PDF

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CN112021318A
CN112021318A CN202010852390.0A CN202010852390A CN112021318A CN 112021318 A CN112021318 A CN 112021318A CN 202010852390 A CN202010852390 A CN 202010852390A CN 112021318 A CN112021318 A CN 112021318A
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pesticide
slow
annular
solution
mixed solution
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张志祥
杨留鹏
徐汉虹
程东美
黄素青
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South China Agricultural University
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South China Agricultural University
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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    • A01N47/28Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
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    • A01N47/38Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< where at least one nitrogen atom is part of a heterocyclic ring; Thio analogues thereof
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Abstract

The invention discloses an annular pesticide slow-release agent, which comprises an elastic ring, wherein the elastic ring comprises the following raw material components, by weight, 0.1-2.0% of a pesticide active agent, 1-10.0% of an organic solvent, 2.15-6.7% of a slow-release material, 5-20.0% of plant essential oil, 0.1-0.5% of an emulsifier, 0.01-0.05% of an organic acid, and the balance of water; the slow release material comprises chitosan, sodium alginate, carboxymethyl chitosan, sodium tripolyphosphate and calcium chloride. The annular pesticide slow-release agent slowly releases the active ingredients of the pesticide under the wet environment or the rain leaching condition, has good control effect on diseases such as corn ear rot and pests such as Spodoptera frugiperda, can obviously improve the control effect of the pesticide, reduces the pesticide dosage, prolongs the control time of the pesticide, and thus protects the production safety of grains.

Description

Annular pesticide slow-release agent and preparation method and application thereof
Technical Field
The invention relates to the technical field of pesticides, in particular to an annular pesticide slow-release agent and a preparation method and application thereof.
Background
Spodoptera frugiperda, also known as fall armyworm, belongs to the genera lepidoptera, noctuidae and spodoptera, is a omnivorous pest native to tropical and subtropical regions of the americas, and larvae can eat 76 and 353 plants of the families, such as corn, sugarcane, sorghum, millet and the like, and spread spreading damage in a plurality of countries. Causing significant losses in brazil and africa. Since 2019, 25 provinces and urban areas of China discover spodoptera frugiperda, the pest-catching area is more than 1500 ten thousand mu, and the actual damage area is 268 ten thousand mu. Researches find that the Spodoptera frugiperda gathers on corn ears to take food as a habit of damage, so that direct yield loss is caused, and the occurrence of plant diseases is aggravated by mixing granular excrement among seeds, so that the yield and the quality of the corn are obviously reduced, and larger economic loss is caused.
At present, the Spodoptera frugiperda is mainly prevented and controlled by chemical agents. However, both manual spraying and unmanned aerial vehicle spraying in the corn heading stage can not effectively prevent and control Spodoptera frugiperda on corn ears, and the traditional spraying causes great waste of pesticide due to drifting of fog drops, and also has certain influence on beneficial organisms such as bees. In addition, the rainfall capacity in south China, especially in the Guangdong area is large, the pesticide is washed by rainwater after being applied, and the quantity of the pesticide which can be really used for preventing and controlling pests is very small, so that a pesticide slow-release agent which can be directionally released and is resistant to rainwater washing is urgently needed for preventing and controlling the pests and the diseases on the corn ears.
Disclosure of Invention
The invention aims to overcome the technical problem that chemical pesticides sprayed on plants in the prior art are easy to scour by rainwater and cannot achieve a real control effect on pests, and provides an annular pesticide slow-release agent which has elasticity, can slowly release insecticidal active ingredients when being bound on the plants in a humid environment or a rainwater leaching condition, has a good control effect on diseases such as maize ear rot and pests such as spodoptera frugiperda, and is safe in grain production.
In order to achieve the purpose, the invention adopts the following technical scheme:
the annular pesticide slow-release agent comprises an elastic ring, wherein the elastic ring comprises the following raw material components in percentage by weight:
pesticide active agent 0.1-2.0%, organic solvent 1-10.0%, slow release material 2.15-6.7%, plant essential oil 5-20.0%, emulsifier 0.1-0.5%, organic acid 0.01-0.05%, and water in balance;
the slow release material comprises chitosan, sodium alginate, carboxymethyl chitosan, sodium tripolyphosphate and calcium chloride.
The annular pesticide slow-release agent disclosed by the invention takes chitosan, sodium alginate, carboxymethyl chitosan, sodium tripolyphosphate and calcium chloride as slow-release materials, can form a three-dimensional network space structure to surround the pesticide active agent, is solid annular and elastic after being prepared into an elastic ring, can be directly tied on plant trees, and can slowly release pesticide active ingredients under a humid environment or a rainwater leaching condition. Meanwhile, tests prove that the pesticide composition has good control effect on diseases such as corn ear rot and pests such as Spodoptera frugiperda. The annular pesticide slow-release agent solves the problem of harm of pests such as Spodoptera frugiperda on plant trees, can obviously improve the insecticidal control effect, reduces the pesticide dosage, prolongs the pesticide control time, and thereby protects the production safety of grains.
Further, the pesticide active agent comprises an insecticide or a bactericide or a mixture of the insecticide and the bactericide; the insecticide is one or a mixture of more than two of chlorantraniliprole, emamectin benzoate, indoxacarb, tetrachlorantraniliprole, high-efficiency cyfluthrin, fenpropathrin, deltamethrin, acephate, lufenuron, chlorfenapyr and dimehypo; the bactericide is one or more of penconazole, tebuconazole, hymexazol, validamycin, thiabendazole, thiophanate-methyl, difenoconazole and carboxin.
Further, the organic solvent is one or more of acetone, dimethyl sulfoxide, N-dimethylacetamide, ethanol, ethylene glycol, ethyl acetate, toluene, xylene, cyclohexanone, hexane, petroleum ether and diethyl ether.
Further, the slow release material comprises, by weight, 0.05-0.3% of chitosan, 1-3% of sodium alginate, 0.05-0.3% of carboxymethyl chitosan, 0.05-0.1% of sodium tripolyphosphate and 1-3% of calcium chloride.
Further, the plant essential oil is one or more of herba Selaginellae essential oil, herba Artemisiae Annuae essential oil, rhizoma Acori Calami essential oil, bergamot oil, birch tar, oleum Lavandula Angustifolia, thyme oil, oleum Cocois, oleum Menthae Dementholatum, herba et flos Pyrethri Cinerariifolii, fructus Amomi rotundus oil, herba Cymbopogonis Citrari oil, oleum Caryophylli, oleum Cinnamomi, folium Eucalypti Globueli, neroli oil and Camphora, herba Chrysanthemum essential oil, wintergreen oil, herba Eupatorii Japonici essential oil, wintergreen oil, tea tree oil, pungent litse fruit oil, oleum Pogostemonis, oleum Menthae Rotundifoli.
Further, the emulsifier is one or more of tween 20, tween 40, tween 60, tween 80, span 20, span 40, span 60 and span 80; the organic acid is acetic acid.
Furthermore, the ring width of the elastic ring is 2cm-10 cm.
The invention also provides a preparation method of the annular pesticide slow-release agent, which comprises the following steps:
preparing raw materials: preparing the raw materials in a formula amount;
dissolving the pesticide active agent: dissolving a pesticide active agent in an organic solvent to obtain a pesticide active agent solution;
dissolving chitosan: dissolving chitosan in organic acid to obtain chitosan solution;
mixing and emulsifying: mixing the pesticide active agent solution and the chitosan solution, and adding an emulsifier to obtain an emulsified mixed solution;
dissolving carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixed solution;
uniformly stirring the emulsified mixed solution and the first mixed solution to obtain a second mixed solution;
adding sodium alginate into water, and stirring to obtain sodium alginate solution;
adding the sodium alginate solution into the second mixed solution, adding the plant essential oil, and uniformly stirring to obtain a third mixed solution;
and adding the third mixed solution into an annular forming groove of a mold, adding water into calcium chloride for dissolving to prepare a calcium chloride solution, adding the calcium chloride solution into the annular forming groove for cross-linking reaction with the third mixed solution, and demolding after curing to obtain the annular pesticide slow-release agent.
Further, the time of the crosslinking reaction is 30-60 min.
The invention also provides an application of the annular pesticide slow-release agent, the annular pesticide slow-release agent is used for preventing and controlling pests on plant trees, and the specific pest prevention and control application method comprises the following steps: the annular pesticide slow-release agent is bound on plant trees.
Compared with the prior art, the invention has the beneficial effects that:
(1) the annular pesticide slow-release agent disclosed by the invention takes chitosan, sodium alginate, carboxymethyl chitosan, sodium tripolyphosphate and calcium chloride as slow-release materials, can form a three-dimensional network space structure to surround a pesticide active agent, is solid annular and elastic after being prepared into an elastic ring, can be tied on plant trees, can slowly release pesticide active ingredients under a humid environment or a rainwater leaching condition, has a good control effect on diseases such as maize ear rot and pests such as Spodoptera frugiperda, can remarkably improve the insecticidal control effect, reduces the pesticide consumption, prolongs the pesticide control time, and thus protects the grain production safety.
(2) The annular pesticide slow-release agent disclosed by the invention is simple in preparation process and low in cost; meanwhile, the annular pesticide slow-release agent is simple and convenient to operate when being applied, a pesticide applying instrument is not needed, and the annular pesticide slow-release agent is sleeved on the target fruits, so that labor and time are saved.
(3) The annular pesticide slow-release agent can accurately act on a control target, accurately control the position to be controlled at a fixed point, has little influence on non-target organisms, and effectively improves the utilization rate of the pesticide.
(4) The product is suitable for areas with large precipitation in south China, and can be used in all weather, rainy days and windy days.
(5) Compared with other pesticide formulations, the annular pesticide slow-release formulation has the advantages that the use amount of organic solvents is reduced in the preparation process, and the residue in the environment is reduced.
Drawings
FIG. 1 is a schematic structural diagram of a mold used in a method for preparing an annular pesticide sustained-release agent according to the present invention;
FIG. 2 is a schematic view showing a state of use of an annular pesticide sustained-release agent of the present invention in a corn ear.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments obtained by a person skilled in the art without making any inventive step are within the scope of the present invention.
Example 1
The annular pesticide slow-release agent is prepared from the following raw materials in percentage by weight: 0.1% of chlorantraniliprole, 2.5% of dimethyl sulfoxide, 4.25% of slow release material, 10.0% of citronella oil, 800.4% of tween, 0.02% of acetic acid and the balance of water.
The slow release material comprises, by weight, 0.1% of chitosan, 2% of sodium alginate, 0.1% of carboxymethyl chitosan, 0.05% of sodium tripolyphosphate and 2% of calcium chloride.
The embodiment also provides a preparation method of the annular pesticide slow-release agent, and the structure of the mould adopted in the preparation method is shown in figure 1. The mold comprises a substrate 10, wherein an annular forming groove 11 is formed in the substrate 10.
The preparation method of the annular pesticide slow-release agent comprises the following specific steps:
(1) preparing raw materials: accurately weighing the following raw materials in percentage by weight: 0.1% of chlorantraniliprole, 2.5% of dimethyl sulfoxide, 4.25% of slow release material, 10.0% of citronella oil, 800.4% of tween, 0.02% of acetic acid and the balance of water. The slow release material comprises, by weight, 0.1% of chitosan, 2% of sodium alginate, 0.1% of carboxymethyl chitosan, 0.05% of sodium tripolyphosphate and 2% of calcium chloride.
(2) Dissolving chlorantraniliprole in dimethyl sulfoxide to obtain a chlorantraniliprole solution, and magnetically stirring for 1-2 h;
(3) adding acetic acid into chitosan for dissolving to obtain chitosan dissolved solution, and magnetically stirring for 1-2 h;
(4) mixing chlorantraniliprole solution and chitosan solution, adding tween 80 to obtain emulsified mixed solution, and magnetically stirring for 1-2 h;
(5) dissolving carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixed solution, and magnetically stirring for 1-2 h;
(6) mixing the emulsified mixed solution and the first mixed solution to obtain a second mixed solution, and magnetically stirring for 1-2 hours;
(7) adding water into sodium alginate, mechanically stirring to obtain sodium alginate solution, and mechanically stirring for 3-5 h;
(8) mixing the sodium alginate solution and the second mixed solution, adding citronella oil, and mechanically stirring for 2-4 h to obtain a third mixed solution;
(9) and adding the third mixed solution into an annular forming groove 11 of a mold through a peristaltic pump, adding water into calcium chloride for dissolving to prepare a calcium chloride solution, adding the calcium chloride solution into the annular forming groove 11 for crosslinking reaction with the third mixed solution for 30min-1h, and washing with ionized water to prepare the annular pesticide slow-release agent with the diameter of 2cm-10 cm.
In this embodiment, the annular pesticide slow-release agent contains 0.18 percent of pesticide active agent by weight, and the pesticide active agent is chlorantraniliprole.
In the embodiment, the application of the annular pesticide slow-release agent is also provided, and the annular pesticide slow-release agent prepared by the embodiment is used for controlling pests on plants. As shown in fig. 2, the ring-shaped pesticide slow-release agent 20 prepared by the embodiment is bound on an ear of corn 30 for controlling pests and diseases of the ear of corn.
Example 2
The annular pesticide slow-release agent is prepared from the following raw materials in percentage by weight: 0.2% of indoxacarb, 6% of acetone, 2.35% of slow-release material, 5% of wintergreen oil, 800.2% of tween, 0.03% of acetic acid and the balance of water.
Wherein, the slow release material comprises 0.15 percent of chitosan, 1 percent of sodium alginate, 0.15 percent of carboxymethyl chitosan, 0.05 percent of sodium tripolyphosphate and 1 percent of calcium chloride according to the total weight percentage of the raw materials.
The embodiment also provides a preparation method of the annular pesticide slow-release agent, and the structure of the mould adopted in the preparation method is shown in figure 1. The mold comprises a substrate 10, wherein an annular forming groove 11 is formed in the substrate 10.
The preparation method of the annular pesticide slow-release agent comprises the following specific steps:
(1) preparing raw materials: accurately weighing the following raw materials in percentage by weight: 0.2% of indoxacarb, 5% of acetone, 2.35% of slow-release material, 5% of wintergreen oil, 800.2% of tween, 0.0.3% of acetic acid and the balance of water. Wherein, the slow release material comprises 0.15 percent of chitosan, 1 percent of sodium alginate, 0.15 percent of carboxymethyl chitosan, 0.05 percent of sodium tripolyphosphate and 1 percent of calcium chloride according to the total weight percentage of the raw materials.
(2) Dissolving indoxacarb in acetone to obtain indoxacarb solution, and magnetically stirring for 1-2 h;
(3) adding acetic acid into chitosan for dissolving to obtain chitosan dissolved solution, and magnetically stirring for 1-2 h;
(4) mixing the indoxacarb solution and the chitosan solution, adding tween 80 to obtain an emulsified mixed solution, and magnetically stirring for 1-2 h;
(5) dissolving carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixed solution, and magnetically stirring for 1-2 h;
(6) mixing the emulsified mixed solution and the first mixed solution to obtain a second mixed solution, and magnetically stirring for 1-2 hours;
(7) adding water into sodium alginate, mechanically stirring to obtain sodium alginate solution, and mechanically stirring for 3-5 h;
(8) mixing the sodium alginate solution and the second mixed solution, adding wintergreen oil, and mechanically stirring for 2-4 h to obtain a third mixed solution;
(9) and adding the third mixed solution into an annular forming groove 11 of a mold through a peristaltic pump, adding water into calcium chloride for dissolving to prepare a calcium chloride solution, adding the calcium chloride solution into the annular forming groove 11 for crosslinking reaction with the third mixed solution for 30min-1h, washing with ionized water, and preparing the annular pesticide slow-release agent with the diameter of 2cm-10 cm.
In the embodiment, the annular pesticide slow-release agent contains 0.37 percent of pesticide active agent by weight percent, and the pesticide active agent is indoxacarb.
Example 3
The annular pesticide slow-release agent is prepared from the following raw materials in percentage by weight: 0.5% of tetrachloro-zoon amide, 2% of dimethyl sulfoxide, 4.0% of slow release material, 15% of litsea cubeba oil, 0.5% of tween 80 and span 80(2:1), 0.05% of acetic acid and the balance of water.
Wherein, the slow release material comprises 0.2 percent of chitosan, 1.5 percent of sodium alginate, 0.2 percent of carboxymethyl chitosan, 0.1 percent of sodium tripolyphosphate and 2 percent of calcium chloride according to the total weight percentage of the raw materials.
The embodiment also provides a preparation method of the annular pesticide slow-release agent, and the structure of the mould adopted in the preparation method is shown in figure 1. The mold comprises a substrate 10, wherein an annular forming groove 11 is formed in the substrate 10.
The preparation method of the annular pesticide slow-release agent comprises the following specific steps:
(1) preparing raw materials: accurately weighing the following raw materials in percentage by weight: 0.5% of tetrachloro-zoon amide, 2% of dimethyl sulfoxide, 4.0% of slow release material, 15% of litsea cubeba oil, 0.5% of tween 80 and span 80(2:1), 0.05% of acetic acid and the balance of water. Wherein, the slow release material comprises 0.2 percent of chitosan, 1.5 percent of sodium alginate, 0.2 percent of carboxymethyl chitosan, 0.1 percent of sodium tripolyphosphate and 2 percent of calcium chloride according to the total weight percentage of the raw materials.
(2) Dissolving tetrachloro insect amide in dimethyl sulfoxide to obtain tetrachloro insect amide solution, and magnetically stirring for 1-2 h;
(3) adding acetic acid into chitosan for dissolving to obtain chitosan dissolved solution, and magnetically stirring for 1-2 h;
(4) mixing the tetrachloro-tetramat dissolved solution and the chitosan dissolved solution, adding tween 80 and span 80 to obtain an emulsified mixed solution, and magnetically stirring for 1-2 h;
(5) dissolving carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixed solution, and magnetically stirring for 1-2 h;
(6) mixing the emulsified mixed solution and the first mixed solution to obtain a second mixed solution, and magnetically stirring for 1-2 hours;
(7) adding water into sodium alginate, mechanically stirring to obtain sodium alginate solution, and mechanically stirring for 3-5 h;
(8) mixing the sodium alginate solution and the second mixed solution, adding litsea cubeba oil, and mechanically stirring for 2-4 h to obtain a third mixed solution;
(9) and adding the third mixed solution into an annular forming groove 11 of a mold through a peristaltic pump, adding water into calcium chloride for dissolving to prepare a calcium chloride solution, adding the calcium chloride solution into the annular forming groove 11 for crosslinking reaction with the third mixed solution for 30min-1h, washing with ionized water, and preparing the annular pesticide slow-release agent with the diameter of 2cm-10 cm.
In the embodiment, the annular pesticide slow-release agent contains 0.95 percent of pesticide active agent by weight percent, and the pesticide active agent is tetrachloro insect amide.
Example 4
The annular pesticide slow-release agent is prepared from the following raw materials in percentage by weight: high-efficiency cyhalothrin 0.2%, ethyl acetate 2.5%, slow release material 4.6%, cinnamon oil 12.5%, tween 800.3%, acetic acid 0.04%, and the balance of water. Wherein, the slow release material comprises 0.2 percent of chitosan, 2 percent of sodium alginate, 0.3 percent of carboxymethyl chitosan, 0.1 percent of sodium tripolyphosphate and 2 percent of calcium chloride according to the total weight percentage of the raw materials.
The embodiment also provides a preparation method of the annular pesticide slow-release agent, and the structure of the mould adopted in the preparation method is shown in figure 1. The mold comprises a substrate 10, wherein an annular forming groove 11 is formed in the substrate 10.
The preparation method of the annular pesticide slow-release agent comprises the following specific steps:
(1) accurately weighing various raw materials: high-efficiency cyhalothrin 0.2%, ethyl acetate 2.5%, slow release material 4.6%, cinnamon oil 12.5%, tween 800.3%, acetic acid 0.04%, and the balance of water.
(2) Dissolving the high-efficiency cyhalothrin in ethyl acetate to obtain a high-efficiency cyhalothrin dissolving solution, and magnetically stirring for 1-2 h;
(3) adding acetic acid into chitosan for dissolving to obtain chitosan dissolved solution, and magnetically stirring for 1-2 h;
(4) mixing the chitosan solution and the efficient cyhalothrin solution, adding tween 80 to obtain an emulsified mixed solution, and magnetically stirring for 1-2 h;
(5) dissolving carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixed solution, and magnetically stirring for 1-2 h;
(6) mixing the emulsified mixed solution and the first mixed solution to obtain a second mixed solution, and magnetically stirring for 1-2 hours;
(7) adding water into sodium alginate, mechanically stirring to obtain sodium alginate solution, and mechanically stirring for 3-5 h;
(8) mixing the sodium alginate solution and the second mixed solution, adding cinnamon oil, and mechanically stirring for 2-4 h to obtain a third mixed solution;
(9) and adding the third mixed solution into an annular forming groove 11 of a mold through a peristaltic pump, adding water into calcium chloride for dissolving to prepare a calcium chloride solution, adding the calcium chloride solution into the annular forming groove 11 for crosslinking reaction with the third mixed solution for 30min-1h, washing with ionized water, and preparing the annular pesticide slow-release agent with the diameter of 2cm-10 cm.
In the embodiment, the annular pesticide slow-release agent contains 0.36 percent of pesticide active agent by weight percentage, and the pesticide active agent is lambda-cyhalothrin.
Example 5
The annular pesticide slow-release agent is prepared from the following raw materials in percentage by weight: deltamethrin 0.1%, dimethylbenzene 2.5%, slow-release material 5.35%, clove oil 7.5%, tween 80 and tween 60(1:1) 0.3%, acetic acid 0.05% and the balance of water.
Wherein, the slow release material comprises 0.1 percent of chitosan, 3 percent of sodium alginate, 0.2 percent of carboxymethyl chitosan, 0.05 percent of sodium tripolyphosphate and 2 percent of calcium chloride according to the total weight percentage of the raw materials.
The embodiment also provides a preparation method of the annular pesticide slow-release agent, and the structure of the mould adopted in the preparation method is shown in figure 1. The mold comprises a substrate 10, wherein an annular forming groove 11 is formed in the substrate 10.
The preparation method of the annular pesticide slow-release agent comprises the following specific steps:
(1) accurately weighing various raw materials: deltamethrin 0.1%, dimethylbenzene 2.5%, slow-release material 5.35%, clove oil 7.5%, tween 80 and tween 60(1:1) 0.3%, acetic acid 0.05% and the balance of water.
(2) Dissolving deltamethrin in xylene to obtain deltamethrin solution, and magnetically stirring for 1-2 h;
(3) adding acetic acid into chitosan for dissolving to obtain chitosan dissolved solution, and magnetically stirring for 1-2 h;
(4) mixing deltamethrin solution and chitosan solution, adding Tween 80 and Tween 60(1:1) to obtain emulsified mixed solution, and magnetically stirring for 1-2 h;
(5) dissolving carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixed solution, and magnetically stirring for 1-2 h;
(6) mixing the emulsified mixed solution and the first mixed solution to obtain a second mixed solution, and magnetically stirring for 1-2 hours;
(7) adding water into sodium alginate, mechanically stirring to obtain sodium alginate solution, and mechanically stirring for 3-5 h;
(8) mixing the sodium alginate solution and the second mixed solution, adding clove oil, and mechanically stirring for 2-4 h to obtain a third mixed solution;
(9) and adding the third mixed solution into an annular mould through a peristaltic pump, adding a calcium chloride solution, crosslinking for 30min-1h, and washing with ionized water to prepare the annular pesticide slow-release agent with the diameter of 2cm-10 cm.
The annular pesticide slow-release agent obtained by the embodiment is an annular pesticide slow-release agent containing 0.17% of deltamethrin.
Example 6
An annular pesticide slow release agent comprises the following raw materials in percentage by weight: 0.5% of penconazole, 1.0% of toluene, 4.5% of slow release material, 10% of calamus essential oil, 800.4% of tween, 0.01% of acetic acid and the balance of water.
The slow release material comprises, by weight, 0.2% of chitosan, 2% of sodium alginate, 0.2% of carboxymethyl chitosan, 0.1% of sodium tripolyphosphate and 2% of calcium chloride.
The embodiment also provides a preparation method of the annular pesticide slow-release agent, and the structure of the mould adopted in the preparation method is shown in figure 1. The mold comprises a substrate 10, wherein an annular forming groove 11 is formed in the substrate 10.
The preparation method of the annular pesticide slow-release agent comprises the following specific steps:
(1) accurately weighing various raw materials: 0.5% of penconazole, 1.0% of toluene, 4.5% of slow release material, 10% of calamus essential oil, 800.4% of tween, 0.01% of acetic acid and the balance of water.
(2) Dissolving penconazole in toluene to obtain penconazole dissolving solution, and magnetically stirring for 1-2 h;
(3) adding acetic acid into chitosan for dissolving to obtain chitosan dissolved solution, and magnetically stirring for 1-2 h;
(4) mixing the penconazole dissolved solution and the chitosan dissolved solution, adding tween 80 to obtain an emulsified mixed solution, and magnetically stirring for 1-2 h;
(5) dissolving carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixed solution, and magnetically stirring for 1-2 h;
(6) mixing the emulsified mixed solution and the first mixed solution to obtain a second mixed solution, and magnetically stirring for 1-2 hours;
(7) adding water into sodium alginate, mechanically stirring to obtain sodium alginate solution, and mechanically stirring for 3-5 h;
(8) mixing the sodium alginate solution with the second mixed solution, adding calamus essential oil, and mechanically stirring for 2-4 h to obtain a third mixed solution;
(9) and adding the third mixed solution into an annular forming groove 11 of a mold through a peristaltic pump, adding water into calcium chloride for dissolving to prepare a calcium chloride solution, adding the calcium chloride solution into the annular forming groove 11 for crosslinking reaction with the third mixed solution for 30min-1h, washing with ionized water, and preparing the annular pesticide slow-release agent with the diameter of 2cm-10 cm.
The annular pesticide slow-release agent of penconazole with the pesticide active agent content of 0.8% is prepared by the embodiment.
Example 7
The annular pesticide slow-release agent is prepared from the following raw materials in percentage by weight: 0.5% of difenoconazole, 1.0% of acetone, 4.9% of slow release material, 6% of bergamot oil, 0.5% of tween 80 and span 80(3:1), 0.05% of acetic acid and the balance of water.
The slow release material comprises, by weight, 0.4% of chitosan, 2% of sodium alginate, 0.4% of carboxymethyl chitosan, 0.1% of sodium tripolyphosphate and 2% of calcium chloride.
The embodiment also provides a preparation method of the annular pesticide slow-release agent, and the structure of the mould adopted in the preparation method is shown in figure 1. The mold comprises a substrate 10, wherein an annular forming groove 11 is formed in the substrate 10.
The preparation method of the annular pesticide slow-release agent comprises the following specific steps:
(1) accurately weighing various raw materials: 0.5% of difenoconazole, 1.0% of acetone, 4.9% of slow release material, 6% of bergamot oil, 0.5% of tween 80 and span 80(3:1), 0.05% of acetic acid and the balance of water.
(2) Dissolving difenoconazole in toluene to obtain a difenoconazole dissolving solution, and magnetically stirring for 1-2 h;
(3) adding acetic acid into chitosan for dissolving to obtain chitosan dissolved solution, and magnetically stirring for 1-2 h;
(4) mixing the difenoconazole dissolved solution and the chitosan dissolved solution, adding Tween 80 and span 80(3:1) to obtain an emulsified mixed solution, and magnetically stirring for 1-2 h;
(5) dissolving carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixed solution, and magnetically stirring for 1-2 h;
(6) mixing the emulsified mixed solution and the first mixed solution to obtain a second mixed solution, and magnetically stirring for 1-2 hours;
(7) adding water into sodium alginate, mechanically stirring to obtain sodium alginate solution, and mechanically stirring for 3-5 h;
(8) mixing the sodium alginate solution and the second boiling solution, adding bergamot oil, and mechanically stirring for 2-4 h to obtain a third mixed solution;
(9) and adding the third mixed solution into an annular forming groove 11 of a mold through a peristaltic pump, adding water into calcium chloride for dissolving to prepare a calcium chloride solution, adding the calcium chloride solution into the annular forming groove 11 for crosslinking reaction with the third mixed solution for 30min-1h, washing with ionized water, and preparing the annular pesticide slow-release agent with the diameter of 2cm-10 cm.
In the embodiment, the annular pesticide slow-release agent contains 1.60 percent of pesticide active agent by weight percent, and the pesticide active agent is difenoconazole.
Example 8
The annular pesticide slow-release agent is prepared from the following raw materials in percentage by weight: 1% of thiophanate methyl, 5% of acetone, 2.75% of a slow release material, 5% of thyme oil, 800.5% of tween, 0.04% of acetic acid and the balance of water.
Wherein, the slow release material comprises 0.1 percent of chitosan, 1.5 percent of sodium alginate, 0.1 percent of carboxymethyl chitosan, 0.05 percent of sodium tripolyphosphate and 1 percent of calcium chloride according to the total weight percentage of the raw materials.
The embodiment also provides a preparation method of the annular pesticide slow-release agent, and the structure of the mould adopted in the preparation method is shown in figure 1. The mold comprises a substrate 10, wherein an annular forming groove 11 is formed in the substrate 10.
The preparation method of the annular pesticide slow-release agent comprises the following specific steps:
(1) accurately weighing 1% of methyl thiophanate, 5% of acetone, 2.75% of slow release material, 5% of thyme oil, 800.5% of tween, 0.04% of acetic acid and the balance of water.
(2) Dissolving thiophanate methyl in dimethyl sulfoxide to obtain thiophanate methyl solution, and magnetically stirring for 1-2 h;
(3) adding acetic acid into chitosan for dissolving to obtain chitosan dissolved solution, and magnetically stirring for 1-2 h;
(4) mixing thiophanate methyl solution and chitosan solution, adding tween 80 to obtain emulsified mixed solution, and magnetically stirring for 1-2 h;
(5) dissolving carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixed solution, and magnetically stirring for 1-2 h;
(6) mixing the emulsified mixed solution and the first mixed solution to obtain a second mixed solution, and magnetically stirring for 1-2 hours;
(7) adding water into sodium alginate, mechanically stirring to obtain sodium alginate solution, and mechanically stirring for 3-5 h;
(8) mixing the sodium alginate solution and the second mixed solution, adding thyme oil, and mechanically stirring for 2-4 h to obtain a third mixed solution;
(9) and adding the third mixed solution into an annular forming groove 11 of a mold through a peristaltic pump, adding water into calcium chloride for dissolving to prepare a calcium chloride solution, adding the calcium chloride solution into the annular forming groove 11 for crosslinking reaction with the third mixed solution for 30min-1h, washing with ionized water, and preparing the annular pesticide slow-release agent with the diameter of 2cm-10 cm.
In the embodiment, the annular pesticide slow-release agent contains 1.93 percent of pesticide active agent by weight, and the pesticide active agent is thiophanate methyl.
Example 9
The annular pesticide slow-release agent is prepared from the following raw materials in percentage by weight: 0.2% of validamycin, 2% of dimethyl sulfoxide, 3.65% of slow release material, 5% of thyme oil, 800.5% of tween, 0.01% of acetic acid and the balance of water.
Wherein, the slow release material comprises 0.05 percent of chitosan, 1.5 percent of sodium alginate, 0.05 percent of carboxymethyl chitosan, 0.05 percent of sodium tripolyphosphate and 2 percent of calcium chloride according to the total weight percentage of the raw materials.
The embodiment also provides a preparation method of the annular pesticide slow-release agent, and the structure of the mould adopted in the preparation method is shown in figure 1. The mold comprises a substrate 10, wherein an annular forming groove 11 is formed in the substrate 10.
The preparation method of the annular pesticide slow-release agent comprises the following specific steps:
(1) accurately weighing 0.2% of validamycin, 2% of dimethyl sulfoxide, 3.65% of slow release material, 5% of thyme oil, 800.5% of tween, 0.01% of acetic acid and the balance of water.
(2) Dissolving validamycin in dimethyl sulfoxide to obtain validamycin solution, and magnetically stirring for 1-2 h;
(3) adding acetic acid into chitosan for dissolving to obtain chitosan dissolved solution, and magnetically stirring for 1-2 h;
(4) mixing the validamycin solution and the chitosan solution, adding tween 80 to obtain an emulsified mixed solution, and magnetically stirring for 1-2 hours;
(5) dissolving carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixed solution, and magnetically stirring for 1-2 h;
(6) mixing the emulsified mixed solution and the first mixed solution to obtain a second mixed solution, and magnetically stirring for 1-2 hours;
(7) adding water into sodium alginate, mechanically stirring to obtain sodium alginate solution, and mechanically stirring for 3-5 h;
(8) mixing the sodium alginate solution and the second mixed solution, adding thyme oil, and mechanically stirring for 2-4 h to obtain a third mixed solution;
(9) and adding the third mixed solution into an annular forming groove 11 of a mold through a peristaltic pump, adding water into calcium chloride for dissolving to prepare a calcium chloride solution, adding the calcium chloride solution into the annular forming groove 11 for crosslinking reaction with the third mixed solution for 30min-1h, washing with ionized water, and preparing the annular pesticide slow-release agent with the diameter of 2cm-10 cm.
In the present embodiment, the ring-shaped pesticide sustained-release agent contains 0.34% by weight of the pesticide active agent, which is validamycin.
Example 10
The annular pesticide slow-release agent is prepared from the following raw materials in percentage by weight: tebuconazole 0.2%, toluene 4%, slow release material 3.3%, artemisia pigweed essential oil 5%, tween 800.5%, acetic acid 0.02%, and the balance of water.
The slow release material comprises, by weight, 0.1% of chitosan, 1% of sodium alginate, 0.1% of carboxymethyl chitosan, 0.1% of sodium tripolyphosphate and 2% of calcium chloride.
The embodiment also provides a preparation method of the annular pesticide slow-release agent, and the structure of the mould adopted in the preparation method is shown in figure 1. The mold comprises a substrate 10, wherein an annular forming groove 11 is formed in the substrate 10.
The preparation method of the annular pesticide slow-release agent comprises the following specific steps:
(1) accurately weighing various raw materials including tebuconazole 0.2%, toluene 4%, slow release material 3.3%, artemisia pigweed essential oil 5%, tween 800.5%, acetic acid 0.02% and the balance of water.
(2) Dissolving tebuconazole in dimethyl sulfoxide to obtain tebuconazole solution, and magnetically stirring for 1-2 h;
(3) adding acetic acid into chitosan for dissolving to obtain chitosan dissolved solution, and magnetically stirring for 1-2 h;
(4) mixing the tebuconazole dissolved solution and the chitosan dissolved solution, adding tween 80 to obtain an emulsified mixed solution, and magnetically stirring for 1-2 hours;
(5) dissolving carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixed solution, and magnetically stirring for 1-2 h;
(6) mixing the emulsified mixed solution and the first mixed solution to obtain a second mixed solution, and magnetically stirring for 1-2 hours;
(7) adding water into sodium alginate, mechanically stirring to obtain sodium alginate solution, and mechanically stirring for 3-5 h;
(8) mixing the sodium alginate solution and the second mixed solution, adding thyme oil, and mechanically stirring for 2-4 h to obtain a third mixed solution;
(9) and adding the third mixed solution into an annular forming groove 11 of a mold through a peristaltic pump, adding water into calcium chloride for dissolving to prepare a calcium chloride solution, adding the calcium chloride solution into the annular forming groove 11 for crosslinking reaction with the third mixed solution for 30min-1h, washing with ionized water, and preparing the annular pesticide slow-release agent with the diameter of 2cm-10 cm.
In the embodiment, the annular pesticide slow-release agent contains 0.36 percent of pesticide active agent by weight percent, and the pesticide active agent is tebuconazole.
Field test 1
The annular pesticide slow-release agent prepared in the embodiment 1 to 5 and a certain brand of chlorantraniliprole suspending agent, chlorantraniliprole and chlorfenapyr suspending agent in the market are used for controlling the corn field for the test of the Spodoptera frugiperda spike pest.
The application method comprises the following steps:
the pesticide is applied for 1 time, three preparations of chlorantraniliprole suspending agent, chlorantraniliprole and chlorfenapyr suspending agent are sprayed, and the annular pesticide slow-release agent is manually sleeved on the position of the corn ear.
The investigation method comprises the following steps:
after each cell is divided, the damage condition of the corn ears at each point is investigated by a Z-shaped five-point sampling method, 3 cells are investigated by each treatment, 20 plants are investigated randomly at each point, and 100 plants are investigated in total in each cell. If living Spodoptera frugiperda is found in the corn ear, the strain is marked as a damaged strain. Recording the number of damaged plants in each corn field, recording the number of live insects in corn ears, and calculating the pesticide effect according to the GB/T17980.6-2000 standard:
Figure BDA0002645171760000181
in the formula, CK represents the damaged spike rate of the blank control area; PT-agent treatment area damage spike rate.
Figure BDA0002645171760000182
In the formula: CK 1-number of viable insects on ear in blank control treatment zone; PT1 number of living insects on ear of drug.
The ear protection control effect is as follows 1:
Figure BDA0002645171760000183
Figure BDA0002645171760000191
as can be seen from Table 1, the ring-shaped pesticide sustained-release agents prepared in examples 1 to 5 have significantly improved ear protection control effects on corn ears as compared to the control treatment agents.
The insecticidal control effect is as follows 2:
Figure BDA0002645171760000192
as can be seen from Table 2, the control effect of the annular pesticide sustained-release agents prepared in examples 1 to 5 on Spodoptera frugiperda was significantly improved as compared with the control treatment agent.
Field test 2
The annular pesticide slow release agent prepared in the embodiment 6-10 is used for preventing and treating corn field for a test with corn ear rot by being mixed with a certain brand of 10% penconazole missible oil, 36% thiophanate methyl suspending agent and 5% validamycin aqua in the market.
The application method comprises the following steps:
the pesticide is applied for 1 time, three preparations of 10 percent penconazole missible oil, 36 percent thiophanate methyl suspending agent and 5 percent validamycin aqua are sprayed, and an annular pesticide slow-release agent is manually sleeved at the position of a corn ear.
The investigation method comprises the following steps:
after each cell is divided, the total spike number, the number of the outbreak spikes and the outbreak level in each cell are investigated, the disease index is calculated, and the prevention and treatment effect is calculated according to the disease index of each medicament treatment and the disease index of a blank control group.
The disease condition grading standard is that the 0-grade morbidity is 0; the 1-grade disease incidence area accounts for less than 1% of the total area of the fruit cluster; grade 3, the disease incidence area accounts for 2 to 10 percent of the total area of the clusters; the disease incidence area of 5 grade accounts for 11-25% of the total area of the fruit cluster; the 7-grade disease incidence area accounts for 26-50% of the total area of the clusters; the disease incidence area of grade 9 accounts for 51-100% of the total area of the cluster.
The drug effect calculation method comprises the following steps:
the disease index is Z (number of disease spikes at each level x representative values at each level)/(total number of investigation spikes x highest representative value) x 100;
the control effect (%) [1- (T-To)/(ck-cko) ] × 100.
T and To are the final disease condition and the initial disease condition of the prevention and treatment area respectively; ck. cko is the final and initial disease in the control zone, respectively.
The control effect is shown in the following table 3:
Figure BDA0002645171760000201
Figure BDA0002645171760000211
as can be seen from Table 3, the control effect of the annular pesticide sustained-release agents prepared in examples 6 to 10 on the corn ear rot is significantly improved compared with the control treatment agent.
In conclusion, the annular pesticide slow-release agent disclosed by the invention adopts the natural polymer material as the slow-release agent and the plant essential oil as the repellent or the insecticidal bactericide, so that the problems that in the prior art, the pesticide reaches the ear less, the waste is great, and the pest and disease at the ear are difficult to control are solved, the preparation process is simple, and the cost is low; meanwhile, the annular pesticide slow-release agent is simple and convenient to operate when being applied, and the utilization rate of the pesticide is effectively improved.
The above description is only for the preferred embodiment of the present invention, but the present invention should not be limited to the embodiment and the disclosure of the drawings, and therefore, all equivalent or modifications that do not depart from the spirit of the present invention are intended to fall within the scope of the present invention.

Claims (10)

1. The annular pesticide slow-release agent is characterized by comprising an elastic ring, wherein the elastic ring comprises the following raw material components in percentage by weight:
0.1-2.0% of pesticide active agent, 1-10.0% of organic solvent, 2.15-6.7% of slow release material, 5-20.0% of plant essential oil, 0.1-0.5% of emulsifier, 0.01-0.05% of organic acid and the balance of water;
the slow release material comprises chitosan, sodium alginate, carboxymethyl chitosan, sodium tripolyphosphate and calcium chloride.
2. The annular pesticide slow-release formulation as claimed in claim 1, wherein: the pesticide active agent comprises an insecticide or a bactericide or a mixture of the insecticide and the bactericide; the insecticide is one or a mixture of more than two of chlorantraniliprole, emamectin benzoate, indoxacarb, tetrachlorantraniliprole, high-efficiency cyfluthrin, fenpropathrin, deltamethrin, acephate, lufenuron, chlorfenapyr and dimehypo; the bactericide is one or more of penconazole, tebuconazole, hymexazol, thiophanate methyl, difenoconazole and carboxin.
3. The annular pesticide slow-release formulation as claimed in claim 1, wherein: the organic solvent is one or more of acetone, dimethyl sulfoxide, N-dimethylacetamide, ethanol, ethylene glycol, ethyl acetate, toluene, xylene, cyclohexanone, hexane, petroleum ether and diethyl ether.
4. The annular pesticide slow-release formulation as claimed in claim 1, wherein: the slow release material comprises, by weight, 0.05-0.3% of chitosan, 1-3% of sodium alginate, 0.05-0.3% of carboxymethyl chitosan, 0.05-0.1% of sodium tripolyphosphate and 1-3% of calcium chloride.
5. The annular pesticide slow-release formulation as claimed in claim 1, wherein: the plant essential oil is one or more of herba Selaginellae essential oil, herba Artemisiae Annuae essential oil, rhizoma Acori Calami essential oil, bergamot oil, birch tar oil, oleum Lavandula Angustifolia, thyme oil, oleum Cocois, oleum Menthae Dementholatum, herba et flos Pyrethri Cinerariifolii, fructus Amomi rotundus oil, herba Cymbopogonis Citrari oil, oleum Cinnamomi, folium Eucalypti Globueli, neroli oil and Camphora, herba Chrysanthemum essential oil, wintergreen oil, herba Eupatorii Adenophorae essential oil, wintergreen oil, tea tree oil, fructus Litseae oil, oleum Pogostemonis.
6. The annular pesticide slow-release formulation as claimed in claim 1, wherein: the emulsifier is one or more of tween 20, tween 40, tween 60, tween 80, span 20, span 40, span 60 and span 80; the organic acid is acetic acid.
7. The annular pesticide slow-release formulation as claimed in claim 1, wherein: the ring width of the elastic ring is 2cm-10 cm.
8. A method for preparing the annular pesticide slow-release formulation as claimed in any one of claims 1 to 7, which comprises the following steps:
preparing raw materials: preparing the raw materials in a formula amount;
dissolving the pesticide active agent: dissolving a pesticide active agent in an organic solvent to obtain a pesticide active agent solution;
dissolving chitosan: dissolving chitosan in organic acid to obtain chitosan solution;
mixing and emulsifying: mixing the pesticide active agent solution and the chitosan solution, and adding an emulsifier to obtain an emulsified mixed solution;
dissolving carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixed solution;
uniformly stirring the emulsified mixed solution and the first mixed solution to obtain a second mixed solution;
adding sodium alginate into water, and stirring to obtain sodium alginate solution;
adding the sodium alginate solution into the second mixed solution, adding the plant essential oil, and uniformly stirring to obtain a third mixed solution;
and adding the third mixed solution into an annular forming groove of a mold, adding water into calcium chloride for dissolving to prepare a calcium chloride solution, adding the calcium chloride solution into the annular forming groove for cross-linking reaction with the third mixed solution, and demolding after curing to obtain the annular pesticide slow-release agent.
9. The process for producing the annular pesticide sustained-release agent as set forth in claim 8, characterized in that: the time of the crosslinking reaction is 30-60 min.
10. The use of the annular pesticide slow-release formulation as claimed in any one of claims 1 to 7, characterized in that: the annular pesticide slow-release agent is bound on plants to control pests.
CN202010852390.0A 2020-08-21 2020-08-21 Annular pesticide slow-release agent and preparation method and application thereof Pending CN112021318A (en)

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CN112826825A (en) * 2021-02-09 2021-05-25 杭州市农业科学研究院 Environment-friendly fishery avermectin sustained-release preparation and preparation method and application thereof
CN113016794A (en) * 2021-03-29 2021-06-25 河北农业大学 Preparation method of plant essential oil grain storage insecticidal slow release agent
CN113966838A (en) * 2021-10-14 2022-01-25 恒枫食品科技有限公司 Astaxanthin nanostructure lipid carrier-chitosan gel particle and preparation method thereof
CN113973833A (en) * 2021-10-18 2022-01-28 河南好年景生物发展有限公司 Sustained-release granule containing lufenuron and emamectin benzoate and applied to corn carpopodium for preventing and treating spodoptera frugiperda
CN115176808A (en) * 2022-07-27 2022-10-14 青岛农业大学 Preparation method and application of environment-sensitive chlorantraniliprole sustained-release agent

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CN110771619A (en) * 2019-11-26 2020-02-11 深圳市威必达有害生物防治有限公司 Medicament for killing solenopsis invicta and preparation method thereof
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CN113016794A (en) * 2021-03-29 2021-06-25 河北农业大学 Preparation method of plant essential oil grain storage insecticidal slow release agent
CN113966838A (en) * 2021-10-14 2022-01-25 恒枫食品科技有限公司 Astaxanthin nanostructure lipid carrier-chitosan gel particle and preparation method thereof
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CN113973833A (en) * 2021-10-18 2022-01-28 河南好年景生物发展有限公司 Sustained-release granule containing lufenuron and emamectin benzoate and applied to corn carpopodium for preventing and treating spodoptera frugiperda
CN115176808A (en) * 2022-07-27 2022-10-14 青岛农业大学 Preparation method and application of environment-sensitive chlorantraniliprole sustained-release agent

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